深紫外光刻光学薄膜

深紫外波段是目前常规光学技术的短波极限,随着波长的缩短,深紫外光学薄膜开发面临一系列特殊的问题;而对于深紫外光刻系统这样的典型超精密光学系统来说,对薄膜光学元件提出的要求则更加苛刻。本文主要介绍了适用于深紫外光刻系统的薄膜材料及膜系设计;对薄膜沉积工艺、元件面形保障、大口径曲面均匀性等超精密光学元件的指标保障关键问题进行了讨论;对环境污染与激光辐照特性等光刻系统中薄膜元件环境适应性的重要因素进行了深入分析。以上分析为突破高性能深紫外光刻光学薄膜开发瓶颈,更好地满足深紫外光刻等极高精度光学系统的应用需求指明了方向。     

Novel insights into controlled drug release from coated pellets by confocal Raman microscopy

The development of novel therapeutics with improved efficacy implies increasing complexity of drug delivery systems, which in turn require advanced methods for their analytical characterization. Among these systems, pellets represent upcoming carrier systems, which show several advantages like simplified dosing and improved compliance among children and the aged population. However, rational development of such systems is hampered by the lack of non‐destructive, chemically selective analytical insight into compound distribution and drug release mechanisms. The aim of this study was to evaluate confocal Raman microscopy (CRM) for investigation of coated drug‐loaded pellets based on visualization of compound distribution and elucidation of drug release mechanisms. Three complementary approaches were applied for pellet characterization: analysis of cross sections after bisectioning, non‐invasive visualization of the pellet surface, and virtual cross sectioning in x–z direction. As the surface of such pellets is structured, a complementary approach of optical topography and CRM was applied for three‐dimensional analysis. Based on the individual Raman peak patterns, the drug and excipients forming the matrix of the pellets and the film coating were successfully visualized with high spatial resolution, verifying homogeneous drug distribution and intact polymer coating of the pellet. Further, analysis of the pellets after certain time intervals during drug release testing revealed pore formation in the polymer coating facilitating drug release and preceding drug depletion in the pellets matrix. CRM represents an upcoming technique for analytical characterization of carrier systems and elucidation of their complex drug release mechanisms, thus supporting rational development of novel therapeutics. Copyright © 2016 John Wiley & Sons, Ltd.     

Raman spectroscopy as suitable tool for the field study of recent volcanic environments

In 2013, a portable Raman setup was implemented for on‐site and rear‐base characterization of volcanic products. Silica and rutile rock coatings, sulfate incrustations and speleothems, plagioclase, clinopyroxene, and (Fe, Ti, Cr) oxides lava minerals were identified on the young lava flows of Piton de la Fournaise volcano. These analytical abilities opens the way of in situ study of the first aging and weathering steps of recent lava flows. This paper relates the preliminary results of the field campaign. Three months after the investigation, all the speleothems have naturally disappeared. Copyright © 2016 John Wiley & Sons, Ltd.     

Coupled Strain and Fresnel Response of Photoelastic Coatings at Oblique Incidence

This paper presents a theoretical model and corresponding experimental results of the oblique-incidence response of a luminescent photoelastic coating (LPC). LPCs use a luminescent dye that both partially preserves the stress-modified polarization state and provides high emission signal strength at oblique surface orientations. These characteristics enable the technique to acquire full-field strain separated measurements and principal strain directions, potentially on complex three-dimensional geometries, without the use of supplemental experimental or analytical techniques. Results of a single-layer LPC on a disk in diametral compression are presented to assess a theoretical model and evaluate the measurement sensitivity.

镍过渡层对磁控溅射银自润滑涂层性能的影响

研究了镍(Ni)过渡层对镍基合金718基底上沉积的银自润滑涂层性能的影响.实验结果显示,具有过渡层的银涂层晶粒尺寸变小,晶格参数和晶格应变无明显变化,涂层表面更加致密,缺陷减少.在77～300K热冲击50次后,涂层表面无裂纹、剥落等现象,具有良好的抗热震性能.在常温大气、常温真空和?100°C真空三种下,对涂层的摩擦磨...     

二甲氧基硫代磷酸酯类农药多残留免疫分析方法研究

以二甲氧基硫代磷酸酯类农药为目标,设计合成了系列半抗原及抗原,制备了4种宽谱特异性抗体。研究结果表明,含不饱和烷烃手臂的半抗原所制备的抗体宽谱特异性优于含酰胺键手臂的半抗原所制备的抗体。采用目标待测物的特征次级结构作为包被半抗原可显著提高ELISA检测灵敏度。经条件优化建立的最佳间接竞争ELISA多残留检测方法可同时检测8种常用高毒农药,其检出限(LOD)在2.6～104μg/kg之间,符合相关限量标准要求。生菜样品药物添加平均回收率为73.9%～121.4%;平均相对标准偏差为10.6%～18.4%。菜心样品药物添加平均回收率为80.4%～121.2%;平均相对标准偏差为13.5%～24.4%。方法精密度均达到气相色谱法的检测水平。     

Synthesis and properties of poly(ether ether ketone)-block-sulfonated polybutadiene copolymers for PEM applications

A novel series of sulfonated block copolymers were successfully synthesized by the condensation of modified poly(ether ether ketone) (PEEK) and polybutadiene (PB), followed by the selective post-sulfonation of PB blocks using acetyl sulfate as the sulfonating reagent. The sulfonic acid groups were only attached onto PB segments due to the high reactivity of double bonds to sulfonating reagent. The degree of sulfonation was controlled by changing the feed ratio of sulfonating reagent to block copolymer. PEEK-b-sPB could be easily cast into flexible and transparent membranes. The obtained membranes exhibited good thermal stability and satisfied mechanical properties. Tensile test showed the incorporation of sulfonate groups into PB blocks resulted in an increase in tensile strength and a decrease in elongation at break. TEM images revealed the existence of ionic spherical domains with the average sizes of 50-100 nm. Some of these small domains further aggregated to form large hydrophilic regions. The proton conductivity values were measured in the range of 10⁻² S/cm in water and increased with increasing IEC and temperature.     

Polymeric ionic liquid as a dynamic coating additive for separation of basic proteins by capillary electrophoresis

A simple and economical capillary electrophoresis method has been developed for the analysis of four model basic proteins by employing a polymeric ionic liquid (PIL), poly(1-vinyl-3-butylimidazolium) bromide, as the dynamic coating additive. When a small amount of PIL was present in the background electrolyte, a cationic coating on the inner surface of fused-silica capillary was established. These PIL modified capillaries not only generated a stable reversed electroosmotic flow, but also effectively eliminated the wall adsorption of proteins. Several important parameters such as the PIL concentration in the background electrolyte, pH values and concentrations of the background electrolyte were optimized to improve the separation of basic proteins. Consequently, under the optimum conditions, a satisfied separation of basic proteins with peak efficiencies ranging from 247,000 to 540,000 (plates m⁻¹) had been accomplished within 11 min. The run-to-run RSDs (n = 3) of the migration times for the four basic proteins were all less than 0.37%.     

Development of a sample preparation procedure of sewage sludge samples for the determination of polycyclic aromatic hydrocarbons based on selective pressurized liquid extraction

An automated, simple and sensitive method based on selective pressurized liquid extraction (SPLE) was developed for the analysis of polycyclic aromatic hydrocarbons in sewage sludge samples. The new sample preparation procedure consists of on-line clean-up by inclusion of sorbents in the extraction cell, and combines elevated temperatures and pressures with liquid solvents to achieve fast and efficient removal of target analytes from complex sewage sludge matrices. The effects of various operational parameters (e.g. sample pretreatment, extraction solvent, temperature, pressure, static time, etc.) on the performance of SPLE procedure were carefully investigated, obtaining the best results when SPLE conditions were fixed at 140 °C, 1500 psi, static time of 5 min and n-hexane as extraction solvent. A new programmed temperature vaporization–gas chromatography–tandem mass spectrometry method based on large volume injection (PTV–LVI–GC–MS/MS) was also developed and analytical determinations were performed by high performance liquid chromatography coupled with fluorescence detection and GC–MS/MS. The extraction yields for the different compounds obtained by SPLE ranged from 84.8% to 106.6%. Quantification limits obtained for all of these studied compounds (between 0.0001 and 0.005 μg g⁻¹, dry mass) were well below the regulatory limits for all compounds considered. To test the accuracy of the SPLE technique, the optimized methodology was applied to the analysis of a certified reference material (sewage sludge (BCR088)) and a reference material (sewage sludge (RTC-CNS312-04)), with excellent results.     

Automated stir plate (bar) sorptive extraction coupled to high‐performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons

Automated methods of PDMS/β‐CD/divinylbenzene‐coated stir plate sorptive extraction (SPSE) coupled to HPLC‐fluorescence detector were reported for the first time. Three automation modes, static SPSE, circular flow SPSE and continuous flow SPSE, were evaluated and critically compared with stir bar sorptive extraction by using six polycyclic aromatic hydrocarbons as model analytes. It was found that the operable sample volume for circular flow SPSE and continuous flow SPSE was larger than that for static SPSE. Under the same extraction conditions, continuous flow SPSE exhibited the highest extraction efficiencies in all automated modes and manual stir bar sorptive extraction for the target compounds. Compared with the manual operation (approximately 5–10 min), automated SPSE required a relatively short time (117–180 s) to finish sampling, washing and sample loading. Besides being labor‐saving and time‐saving, automated SPSE has other advantages, such as no time limit and non‐attended operation. The proposed continuous flow PDMS/β‐CD/divinylbenzene‐coated SPSE‐HPLC‐fluorescence detector was successfully applied to environmental water analysis.